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Structural Characterization of Polysilicate Intermediates Formed During Sol-Gel Polymerization

Published online by Cambridge University Press:  25 February 2011

W. G. Klemperer ,
V. V. Mainz ,
S. D. Ramamurthi  and
F. S. Rosenberg
W. G. Klemperer
Affiliation:
School of Chemical Sciences and Materials Research Laboratory, University of Illinois, Urbana, IL 618O1
V. V. Mainz
Affiliation:
School of Chemical Sciences and Materials Research Laboratory, University of Illinois, Urbana, IL 618O1
S. D. Ramamurthi
Affiliation:
School of Chemical Sciences and Materials Research Laboratory, University of Illinois, Urbana, IL 618O1
F. S. Rosenberg
Affiliation:
School of Chemical Sciences and Materials Research Laboratory, University of Illinois, Urbana, IL 618O1
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Abstract

Identification of polysilicate intermediates formed during sol-gel processing of silica gels and glasses is an important step toward understanding the nature of this process on a molecular level. Although capillary gas chromatography using mass spectrometric detection gives the molecular formulas for low molecular weight intermediates [1], this approach is only semi-quantitative and provides no structural information. An improved protocol has been developed that allows structural assignment and quantitative determination of the principal mono- through hexasilicate structural isamers formed by hydrolysis of methanolic tetramethylorthosilicate in the presence of HC1. This protocol combines quenching by diazomethane, fractionation using spinning band column distillation, identification by capillary gas chromatography, and structural characterization using 29Si{1H} NMR techniques (l-pulse, ID-INADEQUATE, and 2D-INADEQUATE) to provide structural assignments and response factors for the components separated by gas chromatography.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 121: Symposium H – Better Ceramics Through Chemistry III , 1988 , 15
Copyright
Copyright © Materials Research Society 1988

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References

REFERENCES

Klemperer, W. G. and Ramamurthi, S. D., Polym. Prepr., Am. Chem. Soc. Div. Polym. Chem. 28, 432 (1987).Google Scholar
2. For recent studies of sol-gel polymerization, see: a) Ultrastructure Processing of Ceramics, Glasses, and Composites, edited by Hench, L. L. and Ulrich, D. R. (John Wiley and Sons, New York, 1984);Google Scholar
b) Better Ceramics Through Chemistry, edited Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Mater. Res. Proc. 32, Elsevier, New York, 1986);Google Scholar
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3. Klemperer, W. G. and Ramamurthi, S. D., these Proceedings.Google Scholar
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